DE1571404A1 - Process for the production of porous, clay-free, high-temperature-resistant molded parts - Google Patents

Description

DTEiAiIIT NOBEL AiCTIEITGBSELLSCHAPT

Troisdorf / District Cologne 1571404

Process for the production of porous, clay-free, high-temperature-resistant Molded parts. (Addition to the patent application "./Alctenz" D 46 949 VIb / 80b)

Subject of the patent application _β .ο «...“. «/ Aktenzeichen D 46 949 VI" b / 80 b is a process for the production of porous, clay-free, high-temperature-resistant standard parts with high specific surface areas and high abrasion resistance, which is characterized by the fact that fire-resistant oxides with hydroxides of aluminum with the addition of ! atthydrolysierten mixtures of metal alkoxides * bzwo the 3o and 4. flauptgruppe and 4ο iJebengruppe of the periodic table in a conventional Y / else formed of condensed mixed metal alcoholates into blanks, dried and calcined at 150 - 135o ⁰ G, preferably at 300-700 ⁰ G burns.

In an advantageous embodiment of this process, catalytically active metals or their compounds or other connections of the transition elements can also be built into the molded parts, which are suitable as contacts for a number of catalytic reactions.

Gs iat known to make contacts by on a / "self-dead Trüg *" ". Material, such as clay, bentonite Q. the kaolins, catalytically active substances

.009819 / 0806 ^J.

BATHROOM ORIGINAL - 2 -

-a »157140A

applies by impregnation. Contacts made like this they are also used, for example, for oxychlorination reactions ... then generally have a particularly high value Abrasion if the reaction is carried out as a fluidized bed process. Also the activity of the contacts is often carried out Reduced volatility of the catalytically active components. In order to maintain the same activity of the contact used, it is therefore necessary to add fresh contact · Due to the high abrasion the contacts constantly need larger ones!. 'narrow finer Parts are discharged from the reaction system. As is well known, the turnover depends on the one hand on the specific surface of the contact masses and on the other hand duroh the impregnation with the catalytically active Substances, the specific surface of the carrier material is usually reduced, there is a lively interest in to establish highly active contacts that are not burdened by these material parts.

In further development of the process for the production of porous, clay-free, high-temperature-resistant standard parts with high specific surface areas and high abrasion resistance according to patent application. ·· ..... / file number, D 46 949 VIb / 80b made from molding compounds to which catalytically active metal compounds are added before shaping can, has now surprisingly been found that one also particularly effective contacts according to this procedure can produce, inde: a one the catalytically active .'-,

00981 * 9/0804 '

IAD ORIGINAL

Connection of the transition elements with an ordinal number up to 80 used in the form of alcoholates. The alcoholates in particular have been used to carry out the process the following metals as particularly favorable from the mentioned Group exposedί copper, silver, gold, mercury, Vanadium, chromium, molybdenum, tungsten, iron and nickel. The alcohol residue of the metal alcoholate is for the implementation of the method according to the invention without great importance In the case of particularly high-boiling alcohols, this can increase the porosity both aliphatic, fatty aromatic and similar residues to be used·

The porous, clay-free, high-temperature-resistant molded parts that can be used as contacts are ideally suited for catalytic reactions and especially for fluidized light processes, because the catalytically active element is simply built into the ¹ structure of the contact during the production of the molded body an extremely fine distribution and, on the other hand, a * firm anchoring of the kaiElytic element in the carrier material, which also has the consequence that volatilization or loss due to mechanical abrasion of the catalytically active element is very strongly suppressed. While in the impregnation process the catalytically active element is collected in certain layers on the surface of the contact carrier, the active component is in the process according to the invention

19/0804

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Contact before, so that even with abrasion the Aktivi Surface unit even over a long period of time remain.

The anhydrolyzed alcoholate mixture used was prepared as follows!

1 mole of tetraethylsilicate, 1 mole of aluminum sea-butoxide and 1 mol of copper (III) ethylate were mixed with 2 mol | [ajBftjer at Räum empex-atur anhydrolyzed and without further

Treatment used directly as a binding agent "

009819/0804 - 5 -

To increase the activity, the molding compounds * bhbs »ü <..> ., ■

the alcoholates of the catalytically active Uebe] " also in powder form e * oxides or metals added

Instead of the oxides mentioned, self-explanatory

Such compounds are also added to the molding compositions which disintegrate into oxides when burning.

The execution of the method according to the invention wiaJl ^,

■■ ν *

illustrated by the following examples

Example ii

30 parts by weight of fine corundum with a value of less than 20 ^ u (40} 6 times 5 μ) were sprayed with 15 parts of an anhydrolyzed alcoholate by means of a nozzle device and in a mixer by a rotating movement where. small balls with a diameter of 0.3-0.7 works.

The catalyst granules prepared as described above were initially slowly heated to 300 * 0, and with such a heating rate that a bursting of the beads was avoided predried grains were then fired for 6 hours at 300 ° C. The resulting catalyst grains have a specific surface area of 180 m * / g. The alcoholates used as binders are converted into almost pure oxides by the firing process together with the alumina hydrate.

They were previously mentioned using catalyst grains used with good success in an ozychlorination reaction in which ethylene, hydrogen chloride and air are added Ethylene dichloride were implemented.

Example 2:

25 parts by weight of fine corundum in a particle size distribution which corresponded to that of Example 1, 65 parts by weight of alumina hydrate and 10 parts by weight Copper (II) oxide were with 15 parts by weight of the binder described under 1 on the basis of Tetraethylsilicate, aluminum · ec.-butylate and copper (II) ethylate sprayed. Both the pre-drying and Firing was also carried out according to Example 1.

This catalyst could also be used with good success for the above-mentioned oxychlorination reaction insert. Sa · in the contact particles first in Fon The copper present in its oxide is replaced by the gaseous salic acid in the start-up phase of the reaction

009819/08 (K

- Cr - ■,

157H0A

di · katalytiach-wirkaaaan copper chloride · converted ·

O0SL819 / 080A

Claims (1)

·. 7 - 1.57H04 Claim 1 · World · Formation of the manufacturing process Clay porous, clay-free, high temperature resistant Format parts, according to patent application / file files D 46 949 VIb / eOb, from molding compounds which can be used to create catalytically active metal compounds, characterized in that «an the molding compounds the more catalytically effective: compounds of the transition elements with an ordinal number up to below 80 added in fora des alcoholates. 2 · The method according to claim 1, characterized in that «to the alcoholate the approach in the preparation of the mixed, condensed metal alcoholates used as a binder is added. 3 · Method according to claims 1 and 2, characterized in that aan uses formats which also include the catalytically effective transition elements in their fora Oxides or, in the form of clay, compounds which are converted into their oxides on burning. 4. Method according to claims 1-3, characterized in that that «used on molding compounds which additionally contain the catalytically active transition elements in finely divided form Sleaente included ^ «. _{4V +} 009819/0804 fat. Pr.Kni./Nie.